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1390

PROCEEDINGS OF THE IEEE, VOL.

59, NO. 10, OCTOBER 1971

Thin-Film Processes for Microelectronic Application


LAWRENCE V. GREGOR

to Abstract-The rapid development the microelectronics industry be fabricated; conversely, the unavailability of sufEiciently stable of over the last decade has placed exceptional demands on thin-film and reproduciblethin-filmmaterials and processes has been a severe pace technology since, t o a large extent,it controls the technological limitation m attempting to utilize G e , GaAs, and other semiconof that industry. This demand has challenged the thin-film techductors m integrated circuits, even though the higher electron nologist t o develop new and improved processes for both thin-film materials appears to offer a performance adand devices as well as for the thin-film conductors insulation needed mobilityinthese by semiconductor devices. The projected demands of the coming vantage. il to decade wl require advances in the technology comparable those of Presently, most thin-filmapplications require either highlyconbe the past decade if the full potential oflarge scale integration is to ductive or insulating materials, although resistive and semiconducachieved. tive films have their uses. These films serve as the basis of passive The variety o f materials and processes required t o mee4 adequately elements, interconnect active elements, protect and insulate various the total needs of the industry has necessitated the development of several depositiontechnologies.Vacuum evaporation, sputtering, portions of the circuit, connect it to the external world, and even chemicalvapordeposition, d i m e n t a t i o n , etc., are all in volume h furnish te active medium ofthe semiconductor itself. Not only are manufacturing use and the technologies of each of these techniques such films used on the semiconductor.s&ace (die or chq level) has been significantly improved during the past ten years. A similar but a s on the chip carrier or substrate in hybrid or thin-film cirlo increase in process capability and control has been necessary in the area of pattern definition in order to allow the development of fine cuit technology (obe defined). Since the technology of magnetic t lineetchingwhich achieves therequirednarrowlinewidths and films is a separate subject in its own right, it will not be considered separations in todays microelectronic assemblies. in this paper. Thin films are not only used as functional elements of The materials of major interest t o t h eindustry as well as the dethe completed device, but are essential in the processing sequence position techniques and photoengraving processes usad intheir which produces the device. Some feeling the variety ofthin-film for processing are highlighted. The discussion includes the status and as limitations of the technology it exists todayas well as a consideramaterials used in microelectronics is given by Table I. tion of the advantages and disadvantages of the various processes The terms monolithic circuits, hybrid circuits, and thinboth as of today and for the future.

INTRODUCTION URING the past decade, advances in semiconductor and thin-film electronics, particularly in the utilization of integratedcircuits,have been limited by theavailabletechnology of thin films more than by any other factor. For this to have meaning, the definition thin films should be stated. Rather of than attempt a functional or intrinsic categorization, a simple physical uf criterion will be employed. A thin film is a s r- layer 5 5 p thick, often much less. This will hopefully avoid the ~ t u r a tendency to l hn associate the termt i film with specific deposition methods, or to narrow the meaning to include only those films used in silicon device and integrated circuit technology. There are many reasons for the widespread use of thin films in microelectronics. Perhaps the most important is that only thin films can be processed to yield the small size, low power,and high circuit density desired. Secondly, films are important in other essential thin processes, e.g., diffusion masking. Also, thin-film deposition techniques allow for convenient production of high-purity substances or materials withclosely controlled composition. Finally, some vital features of present circuitscan only be achieved by using thin films, such as silicon s u r f a c e passivation with SO2. Many other specific arguments can be made for the desirability of thin-film technology, depending on the material in question the function to be achieved. or Although semiconductor electronics today is largely based on silicon and the planar diffwion process, other materials and fabrication methods are finding increasing application. In a striking way, the sUCCeSSful employment (or lack of it) of these materials is dehn pendent on the status of the particular t i film technology associated with the critical process or functional operation of the device. For example, development of special thin-film diffusion masking methods was necessary to enable electroluminescent diode arrays

film circuits are often employedto describe various types of microelectronic components. These will be used in accordance with the following generaldefinitions: Monolithic Circuits: passive and active elementsfabricated in or on the semiconductor surface, with thin-film interconnections and terminals. Hybrid Circuits: passive components and interconnectionsmade from t i or thick films with active devicesattached by a separate hn process step. Thin-Film Circuits: all activeand passive elementsas well as interconnections made fromthin films. All are illustrated in Fig. 1. The emphasisin the ensuing discussion will be on the methods of fabricating and employing thin films in practical microelectronics, with brief survey of some interesting a potential applications which rely on thin films.
hhXOD.3 OF F M L I T I O N I L

Many methods are available for forming s u r f a c e films, and most of them are not recent discoveries.For example, sputtering was observed in the mid-19th century, and vacuum evaporation was an annoyance to the early incandescent lamp manufacturers [l 1. It is convenient to classify thin films by their methods of deposition, realizing that other ordering systems are also possible and useful. It will be seen that, within each general type of film deposition method,there is a wide r n of materials, properties, and a p ap plications. Chemical Reaction This method relies on a chemical reaction between the original surface and its environment to produce a thin layer of a new substance on the surface. The basis the present technologyof silicon of devices and the integrated circuits is the formation of a thin film of SiO, on Si by the following reaction : Si,,,

Manuscript received March 23, 1971; revised May 5, 1971. The author is with IBM Components Division, East Fishkill Facility, Hopewell Junction, N.Y.12533.

+ O2

--*

SiOZ(r).

The resulting amorphous Si02 layer serves to passivate the sur-

GREGOR : THIN-FILM PROCESSES FOR MICROELECTRONICS

1391

TABLE I THIN-FILM MATERIALS M r c ~ o p ~ ~ c m o ~ ~ c s IN


h o r = P

Interconnections/ Insulation/ Terminals Encapsulation Passivation Resistive A1 P,Os A1 alloys Si) (Cu,SiO, cu A1203 Mo-Au Ti-Ag Cr-Ag Pt-Au Cr-CuAu Pb-Sn SiOl Si,N, BN Si0 SiO, SiO, . P,O, A1203 PbO . B,O, . SiO,

Capacitive Ta SiO, Ta,O, PbO TaN Cr S i 0 HfO, NiCr ZrO, SnO, GaAs PbTiO, kanthal polymer

Semiconducting Si

Processing SiO, photopolymer Mo Cr

Development Si,NrSiO,

SeSi
Te Sic GaP AIN

InAs InSb PbS PbTe CdS CdSe ZnSe

Nb,O,
Ge-S+Te ZnO

N+

ISOLATION

SUBCOLLECTOR

TRANSISTOR

SILICON SUBSTRATE

la)

ACTIVE COMPONENT TERM1


CAPACITOR

RESISTOR

SUBSTRATE

outer surface.It is common to assist the process by making the conductor electrically positive with respect to its surroundings. This is then called anodization is widely practiced yield thin oxide and to dielectric films on Ta, V, Nb, and Al. It can also be used to produce films on Si. The film thicknessx is proportional tothe voltage drop V across the film ( x = k V ) and hence can be controlled accurately [ 5 ] . An interesting variation of this process is the conversion of a slowetching film (Si3N4)to SiO, [ 6 ] . In some interesting development programs, a much lower temperature is employedto produce an extremely thin fl (- 25 A) so im that the electron tunneling phenomena can be employed to produce useful effects. The best known devices this time are Josephat son-effect devices usingSnO or PbO [7] and thevariable V, MNOS FET [SI which employs SiO,. A more conventional MOSFET device has been made anodizing an A film over the channel proby I to duce an M2O3gate insulation p].
Chemical Vapor Deposition

(bl

THIN-FILM TRANSISTOR SOURCE,


GATE DRAIN

BISTABLE RESISTOR

PHOTOSENSOR

SUBSTRATE
(Cl

Fig. 1 . Cross-sectional diagram of thethree types of microelectroniccircuits using thin films. (a) Monolithic silicon integrated circuit.(b)Hybrid silicon thin-film circuit. (c) All thin-film integrated circuit.

face of Si [2]. It also functions as a convenient diffusion mask and provides the electrical insulation between the Si and the interconofdifnection lines. The SiO, layer can be formed in a number ferent oxidizing gases, notably H,O, N20,and to a lesser extent, in CO, [3]. Primarily, the reaction is controlled by the rate of diffusion of oxidant across the SiO, film. hence, the growth rate decreases with time. The most general expression which relates the film thickness to oxidation time is [4]
X

+ k,x

= k2t

+ k3

where x is the fl thickness at time t, and k,, k,, k3 are constants im depending on temperature,. oxidizing and silicon crystal orientagas, tion. No other common semiconductor forms a naturally occurring oxide film which useful properties. To a great extent, this is why has silicon is predominant in integrated circuit applications. In thermal oxidation, the oxidant diffuses through the growing film to the oxide-silicon interface. There another class of reactions is in which the opposite reaction occurs: the silicon (or conductor) cation migrates toward and reacts with the oxidizing species at the

This is sometimes called the CVD process it employs either and a chemical reaction between two or more species or a chemical decomposition to produce the desired film. The latter method is somewhat imprecisely referred to as pyrolysis. In these reactions, the surface does not playan active role in the formation of the thin film. All three types of thin fls can be formed by t i method, as im hs exemplikd by the following reactions [lo] : SiH4 0, + SiO, WCI, -b w i-1 3, c SiCI4 + Si + 2C1, . The third chemical reaction is of particular importance.Depending on the surface conditions and crystal structure, the resulting Si film can be singlecrystalor polycrystallinein nature. The former process is called epitaxy and is not usually considered a thin-film process, although most epitaxial silicon films are much less than 5 p thick, and fall within the physical classiliation of thin films. If the film is polycrystalline, as it is on SiO,, then this process is definitely athinfl process. It is widely usedto form the gate electrode in the silicon im self-aligned gateFET process [1 11. The major requirements for a practical CVD process are a suitable compound to cany the desired substances to the surface, a heterogeneous gassolid reaction whose rate is much faster than any competing process, a reactor system to assure. temperature and uniformity, gas composition homogeneity, and a reasonable batch size. Temperature control is important since the reaction is usually thermally activated. The deposition of SiO, is one of the most widely used CVD processes. A number of different chemical systems have been employed: SiH4+0,, Si (OR)4, Cot, etc. In addition to pure Si02, processes havebeen developed to incorporate stabilizing substances

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PROCEEDINGS OF THE EEE, OCTOBER

1971

into the basic SiO, matrix; glassy materials containing P, Al, B, etc., have been deposited as thin films [12]. In addition to polycrystalline Si, number of thin metal films can a be formed by CVD. Both M o and W can be deposited by decomposing their halidesor carbonyl compounds [13]. The substrate temperatures needed forim deposition may often fl be lowered appreciably by supplying RF or microwave energy to create a plasma or glow discharge [14]. Films of SiOz and Si3N4 have been deposited in this way, but reproducible film properties are difEcult to achieve. Vacuum Evaporation If the pressure inside a chamber is reduced sufficiently, substanceswill evaporate; their atoms or molecules will travel in straight trajectories if the pressure is so low that their mean free path is of the same magnitude as the dimensions of the chamber. This is the basic principle of vacuum evaporation. A substance must attain a vaporpressureof torr to deposit at a useful rate [15]. For most materials, this means an elevated source temperature is necessary. The rate of film growth depends on the rate of arrival of evap orant particles and the probability of a given particle being retained on the surface. The latter is measured by a parameter called the sticking coefficient. Some important factors in vacuum evaporation are the vacuum required, the nucleation of the initial deposit, and the stability of the evaporating substance. The mostsuccessful substances for film formation are elements or simple compounds thin whosevaporpressuresrangefrom 1 to 10 x torr in thetemperature interval 600 to 1200C.The level and composition ofbackground gases are kportant if the film properties are sensitive to impurity atoms. A great deal of investigationhas gone into appropriate means of maintaining the source of evaporating material at the desired temperature. The earlied sources were refractory metals such as tungsten which could beheated by passage of a dc current. Later, boats of various materials such as molybdenum, graphite, and boron nitride were developed. additionto d r c electrical heating indue In iet tive methods are also in use. By using RF induction and largediameter inert crucibles, evaporation of a numberof different metals of highrates in a single evaporator cycle is possible (Fig. 2). The major problems with this method are the probability of contamination of the deposit by the sourceand source failure. To circumvent these problems,a f o q w d electron b a can be em used to heat a portion of the material. While miniminng contamination and allowing sigdcantly higher temperatures to be attained so that more refractory substances can be evaporated, electronbeam evaporation is more costlyand complex. The radiation from x the source may be a factor in certain applications, such as MOSFET device threshold voltages [16]. The evaporation of alloys is generally more difficultthan pure metals, sincethe different vapor pressures of the elements can lead to fractional distillation during evaporation, and hence vary the film composition. Among the more ingenioussolutions to this problem is the flash evaporation of pellets of the alloy [17]. The use of alloys and mixtures such Cr and Si0 (cermets) is the practical as only film hn way to get sufficiently high resistance to make t i film resistors.

CRYSTAL THICKNESS MONITOR

COMBINATION LIQUID NITROGEN COOLED TRAP AND TITANIUM ADSORPTION PUMP SUBSTRATE FINGER WATER COOLED BAFFLE PLATE R.F. HEATED CRUCIBLE WATER COOLED RADIATION SHIELD SHIELD

WATER COOLED SHUTTER:\y


DUST CAP HOLDER AND

REMOVER

ROTATING SOURCE PLATFORM

Fig. 2. Multiple-source vacuum evaporation system employing RF crucible heating.Bell jar removed to show components.

plasma containing positive ions and electrons. The positive ions could then be accelerated toward the target by the potential drop of several kilovolts.Unfortunately, this technique is not generally useNfor nonconductivetargets, since the accumylated positive charge on the target surface counteracts the applied dc voltage. To circumvent t i difEculty, the application of an RF potential hs This between the electrodes was proposed [18]. method of RF sputtering has recently been developed into a practical deposition process for dielectric films (Si02, A1203, Si3N4)which have many applications [19]. The alternating potential of the RF input sequentially allows the targer surface to be bombarded by positive ions and the positive charge to be neutralized by the highly mobile electrons. The technique can also be applied to metals and semiconductors. If the positive ions used in sputtering are not chemically reactive, such as A ,then little or no change occurs in the r composition of the material from target to film. If, however, a reactive gas is present when the plasma is formed, the target surface can form chemical compounds which then become part of the depositing film. This is known as reactive sputtering, and has been used to produce various films, mainly oxides and nitrides. Likewise, usinga g a s mixture can result ina film of mixed composition, such as silicon oxynitride [20]. Reactive sputtering generally proceeds with a slower rate of deposition than direct sputtering. One of the most significant recent developments has been the recognition that a considerable amount of resputtering of the deim posited fl can occur, with important effects on the resulting film properties [21]. Likewise,a quantity of the sputtering gas may be trapped in the film and can cause variations in the physical and chemical properties of the film [22]. Finally, the development of phenomenological models explain the emission of to material as well as the electrical behavior of a sputtering system [23] allows the technique to be generalized to the point where it is probably applicable to a wider variety of materials, rates of growth, and film properties than any other method.
+

Physical Deposition Certain useful t i films are deposited by simple physical dehn Sputtering position followed by a postdeposition treatment to assure homoThis method is sometimes calledimpact evaporation, since a geneous film properties. The mostcommon example ofthis method surface is bombarded with ionized particles whichtransmit energy is the deposition of a fmely powdered glass (called a frit) from by fusingthelayer at an elevated to the atoms or molecules of the surface so that the most energetic liquidsuspension,followed temperature. This allows the formation of a coherent chemicallyare emitted. The emitted particles then diffuse to an adjacent surface where they build up a thin-film deposit. Originally sputtering stable glass layer on a silicon surface, which protects the devicefrom was applied to conductive materials, since dc potential could be the environment and allows nonhermetic packaging 1241. In conhs established between the target (cathode)and an anode in a gaseous junction with the appropriate terminal metallurgy, t i sealing tech-

FOR GREGOR : THIN-FILM PROCESSES

1393

nique has been found to produce extremely high component re[25]. Unfortunately, the complexglass composiliability in field use tion and relatively high fusion temperature (575C) do not make t i method attractive for integrated circuits which employ siliconhs aluminum contacts or aresensitive to the traces of alkali ions commonly found in glass. Another method which has found increasing use is the deposition of a liquid suspension of appropriate materials followed by conversion to a glass-like film from which dfisants can be s u p plied to the semiconductor. These are often generically referred to as doped-oxide or paint-on sources [26]. The technique combines the the ease of pattern formation with the advantages of planardiffusion process. Some available diffusants are P, B, A s , and Au. One difficulty with this technique is the inability to get a reproducible high surface concentration diffusant. Another is the susceptibility of to deleterious ionic contamination. o For extremely thin dielectric films t be used in tunnelling devices, a specialized technique, based on the Langmuir monolayer adsorption method, employsa monolayer of a fatty acid salt. Films of 25 A of bariumstearate can be superimposed to give insulating films whose thickness is some multiple of the monolayer thickness [27]. In addition to the fatty acid salts, other materials may be prepared for study as thin films,such as chlorophyll-a [28 1.

is encountered. Such instruments are often known by their trade names (Dektak, Taly-Surf). The step height thus directly measured is the film thickness. Ofcourse, only the thickness the edgecan be at measured. Other more complex methods havebeen developed such as the absorption of beta-particles of known energy.Finally, if the relative dielectricc o n s t a n t of an insulatingfilm is known, as estimate of thickness be made from the measured capacitance the iilm can of between two suitable electrodes of known area. The latter method, thoughcumbersome, is often useful cross in calibrating other methods. Most of the methods for transparent or translucent films are optical techniques, which utilize either absorption or interference of light to make the measurement. simple rapid method evaluaA for tion of thicknesses of nonabsorbing films is VAMFO (variable amplitude multiple fringe observation), which is suitable for films from several hundredto several thousand angstroms, but requires a relatively large area [34]. An even simpler method is color comparison of thefilm to a calibrated sample with various thicknesses, called a stepgauge. For accuracy, a calibrated sample is required for each material, since the color change due to is interference which is a functionof the refractive indix of the material. For thicker films, opaque films, etc., thickness measurements be madeby multiplecan b a interferometry. Unfortunately, the requirement of a highly em reflecting surface and the need for precision optical equipment make Miscelhous this method more cumbersome. be measured by Very thin films of transparent material may Most of the remaining methodsfor thin film formation are not close to everyday use. The formation of polymerdielectric films by polarization spectrometry or ellipsometry, in which the phase angle interirradiation of adsorbed organic molecules on surfaces was studies shift of elliptically polarized light being reflected back from the extensively in the pastfor applications in cryoelectronic circuits and face ofthe film and substrate is a function of film thickness and refractive index. This method is most useful for extremely thin films for capacitor fabrication [29]. One organic polymer method with from a monolayer toseveral hundred angstraoms. Another meaup potential use is the deposition of poly-pxylylene (called Parylene commercially). This is a chemical-physical method which relies on surement suitable for very thin films is the Brewster-angle technique the thermal cracking of a source material, di-pxylene, to produce for accurate measurement of refractive index [35]. reactive free radicals which repolymerize when impingingon a sur- Structural Properties face [MI. is claimed that this method has been successful in proIt The structural details of thin films of importance governing are in viding environmental protection silicon circuit chips encapsulated to suchbehavior as resistivity,stress,chemical stability, and other in this manner [31]. Other methods which are useful in preparing thin films of electronic interest are theexploding-wire method [32], more subtle properties which will be discussed in more detail along and chemical spraying. latter method is not free from difficulties with reliability. Structural investigations can be simply microscopic The such as powdery deposits, but hasbeen used to make coherentfilms observations of grain size, texture, metallographic structure, staining, etc. However, a large number of thin films are devoid of any ofZnO [33]. visible structure and more refined investigatorytools are employed. CHARACTERIZATION OF THIN F W These include: X-ray and electron diffraction to determine the extent of crystallinestructure in the iilm ;scanning electron microscopy The control ofthin-film properties requires number of methods a iilm. In some cases, t i may be (SEM) to determine high-resolution surface features; transmission hs of measuring the properties of the done even duringdeposition,butmostevaluation is performed electron microscopy (TEM)to detect internal fine structure; preferafterward. The refinement of measurement methods has been re- ential chemical etching; and polarized lightfor internal stress analsponsible for much of the technological advance made the use of ysis. If the substrate is transparent to infrared or visible radiation, in thin filmsin the past decade. The of the discussion deal with the method of internal reflection spectroscopycan be used to study rest will the absorption propertiesof surface films [36]. measurements directly involving the l i l m s themselves.

Thickness

Mechanical Properties

A very basic parameter is the thickness of the film. Its value is predetermined by a knowledge of the deposition or growth rate asa function of the parameters of the deposition system (power, temperature, pressure, etc.). In some cases, the actual thickness canbe measured in situ during deposition. The optical absorption of a transparent film can be monitored during evaporation sputtering. or For other films, indirect rate monitoring methods are used which employpreviouscalibrationofthesystem.However,whenthe process is complete,it is desirable to be able to measure the actual ITlm thickness. This is normally done by physical or optical mt%hods. The simplest physical method employs a sensitive stylus which is allowed to glide overthe surface until the edge of the deposited film

Actually the so-called mechanical properties are really manifestations of the interaction of physical structural factors. Howand ever, they are conveniently discussed as such, and the most significant are probably stress, hardness, and the coefficient of thermal expansion. Stress is particularly important, since the combination of residual intrinsic stress and that due to expansion mismatch can easily exceed the yield strength of the film and/or adhesive forces, resulting in separation or fracture. Both compressive and tensile stress are common. It is generally preferable to have the former to prevent propagating cracks from occurring. Hardnessis a measure of the resistance of the materialto abrasion and scratching. One of the hardest known thin films i silicon nitride [371. The coefficient s

1394
TABLE I1 CWLWATIONOF TYPICAL MICROELECTRONIC THIN-FILM MATERIAL BY R~srsrrvrn m OTHER ELECTRICAL PROPERTIES Film Resistivity Type Example (Q . cm) Parameter Other SiO, Si3N4 tan 6 Dielectric Si0 1018 Si0 & Dielectric 1014 SrTiO HNOS-HF Si Resistor Ni Cr 10 TCR A1 Resistor Cr SiO, Au

PROCEEDINGS OF THE I , E

OCTOBER

197 1

TABLE IV ETCHANT !hLUTlONS FOR C M O FILMS O MN

Mask
KTFR SiO, KPR KPR AZ-1350 AZ-1350 KPR

Etch

H3PO4-HNOs

Mo
~ ~~

Semiconductor Semiconductor Conductor Conductor Conductor

CdS PbTe

10-3

P,
Al-Si

Cr-Si Ta

A l Mo

dwr
ways has an associated space-charge layer whose behavior is nonlinear, but the contact is still ohmic if the space-charge layer impedance is negligible in comparison withthe bulk semiconductor resistance. It is implicitly assumed that minority carrier injection is either absent or negligible, and that trapcharging effects are small. The fabrication of an ohmic contact thus requires that theimpedance ofthe ,Schottky bamer is low. Thereare two current transport mechanisms in Schottky barriers: a) thermionic emission, and b) tunneling. These correspond, respectively, to the two main emcontacts:a) choosing a metal which makes a pirical ways of making low Schottky barrier with the semiconductor,b) doping the semior conductor heavily near the contact so that the barrier will be thin enough to be penetrated easily by tunneling [ a ] .
Chemical Properties

P t

k S barrier height - i

TABLE 111

MBCCHANISMS OF ELECTRICAL CONDUCTION DIELECTRIC PI FILMS


Mechanism
~~~ ~ ~~~

Thickness Range, P
~0.01

Tunneling Emission, Schottky Emission, Frenkel-Poole Space charge limited Ohmic

0.01-0.5 0.01-0.5

1.0

I I I I I

- T -T2 -

Current Dependence

Example GaSe Ta,O, Si3N4 Si0

Vz exp ( - k / v ) exp ( o @ / T ) exp (2aJE/T)


V/X3

Vexp ( - b / T j

The most important propertythin of is their behavior towards s p e d c etchants. This determinestheusefulnessof the Electrical Properties film, for if high-resolution patterns cannot generated chemical be by For microelectronics, the electrical properties of thin films are means, the film is of limited use. The etch rate and the edge resoluis of prime importance.No other single characteristic spans as wide a tion attainable with a particular etching processof great concern. Q . cm for the most The appropriate range as electrical resistivity,rangingfrom etching solutions procedures for some common and conductive film to lo* cm for the least (SiO,). In fact, every thin 6lms are given in Table IV,and data on other materials are s u m type of thin film can be characterized by its resistance and one or marized in the literature [41]. The etch rate is determined by the more other electrical properties. This is illustrated schematically in film structure, density, impurityconcentration, strain, and other Table 11. Recently, considerableattention has been paid to the con- factors. A correlation exists between such properties as etch rate as the duction mechanisms by which thinfilms of dielectric materials ex- and corrosionresistance and observablequantitiessuch hibit measurable electrical currents. These currents are non-ohmic, visible and infrared absorption spectra [42]. Recently, significant advances in instrumental techniques have and the more important processes are tunneling,fieldemission, hr spacecharge-limited current flow, and internal field emission. These been made which allow much e structural detail to be disclosed. wanare shown in Table 1 along with some typical 11 materials. A striking The importantnew techniques of X-ray fluorescence, electron confirmation of the theory of electron tunneling has been found ning chemical analysis(ESCA), and ion source spectrometry (ISS) allow, in effect, a quantitative analysis to be performed on the thin experimentally for GaSe [38]. detectResistive films generally obeya relationship called Mathiessens film. By using X rays, extreme sensitivity may be achieved in ing trace impurities. ESCA allows local analysis of a small area, rule while ISS allows mass-spectrometric chemical analysis a monoa of P = P ( T ) + P G ) + P@) layer of the film.Somewhat older but still useful methods employ which equate the sum of the temperaturedependent p(V,tempera- radioisotopes to study film behavior. These can be introduced exture-independent p(i) resistivities plus the geometry dependent termternally, or generated in the film by neutron activation of natural and counting offilm p@) to the observed resistivity p . By controlling p ( T ) , it is possible isotopes occurringin the film. Selective etching to to get some control of temperature efficient of the resistance (TCR). allows a profile be constructedof the radioactive substance. These In order to bring the values of thin-film resistors to predetermined methods have been useful in the study of the distribution of alkali value, it is often necessary to adjust their resistance values. This is ions and hydrogen in SiO, [43], [MI. An important chemical property of glass films is their ability called trimming. The physical methodsof erosion or removal of resistor material is usually feasible for thin films.A useful tech- to resist diffusion of corrosive substances which can attack internot nique is the thermal pulse trimming resistors. A series of current connections, the semiconductor surface, or underlying oxide surof films pulses are allowed to heat the film, lowering its resistivity in small faces. The ability to protect the edges of metallic is called edge coverage, and is vitally important in production multi-interconof increments until the desired range is obtained [39]. nection level integrated circuits [45]. Recently it has been shown A model for a metal-semiconductor contact, whether ohmic in or not,is a Schottky barrier in series with the spreading resistance that there are inherent reasonsfor the difficulty encountered edge of the bulk semiconductor. The metal-semiconductor contact al- coverage by evaporated films [MI. Metallic films for use in micro-

of thermal expansion is important because of possibly disruptive forces arising from a gross mismatch between films or between films and substrate.

FOR GREGOR : THIN-FTLM PROCESSES

MICROELECTRONICS

1395

TABLE V PROPERTIES OF METAU EMPLOYED AS THIN FILMS Limiting Current Resistivity Density JIAlan x IO Metal

suitable for vacuum deposited films. Unlike the first two principal methods discussed, there is no reliance on the controlled radiation process to form thepattern; all that is required is a physical mask.
Stencil Masking

Stencil masking employs a barrier, or mask, interposed between a particle stream and a surfaceon which theparticles can condense. 1.59 4.0 poor adhesion Silver The pattern formed isthat of the open portions of the mask. Several 4.0 1.67 poor adhesion; corrosion Copper 7.0 2.35 siliconeutectic 370C, poor features of this process are as follows. First, the mean free path of Gold adhesion Secsilicon eutectic 577C, elec-a particle must be long comparedto the mask-surface spacing. Aluminum 0.5 2.65 ond, the sticking coefficient S, of the evaporant material should be ,, tromigration Aluminum 2.0 +Cu close to unity; this implies an upper limit restriction on the surface extremely reactive Magnesium 4.45 temperature. Third, the resolution of the pattern is governedby the 4.51 poor adhesion Rhodium poor adhesion resolution of the mask itself; there are no physical limits (such as 5.3 Indium dacult etching 20.0 5.6 Tungsten diffraction) but there are obvious mechanical limits. Fourth, there 5.7 corrosion susceptibility Molybdenum 10.0 is a topological constraint that a completely connected in twodimenpoor adhesion 9.8 Platinum 55 Titanium sional pattern requires more than one mask. These constraints resulted in the use of masking for pattern generation of materials which be thermally evaporated in a high can torr). The pattern can be defined to a resoluelectronicsare often judgedby such chemicalcriteria as the thermo- vacuum system (c dynamic stability of their oxide (since this is related to adhesion of tion of k0.0125 mm (12.5 p ) as a practical limit over an area of the metal to underlying SOz) or the physical coherence of their more than 25 cm2. In principle, the use of stencil masking can be oxide.Coherent Al,O, actsto passivatealuminum films from extended to a wide variety of materials. In practice, the method is used primarily for metallic films with some employment for difurther oxidation. Copper films, on the other hand, must be proelectric materials such as silicon monoxide. The most complete aptected from formation of CuzO, and molybdenum films have as their most undesirable feature their susceptibilityof oxidation corrosion. plication of stencil masking occurs in the fabrication of cryoeleccircuit may be A summary of some of the more common metals as thin h tronic circuits [50]. In this case, every element of the used by built from a film whose shape is defined stencil masking. is given in Table V. Mask Fabrication PATTERN GENERATION The mostcommon mask materialsare metals and alloys because The fabrication of modem solid-state electronic components of the ease of manufacture and durability. The pattern of openings places great emphasison the generation of accurate high-resolution patterns in thin films of a wide variety of materials. At this point, in the mask can be made in a number of ways. The most common it is well to establish the differences between ti h the so- method is to engrave, drill, or punch out the pattern in a metal hn and called thick h [47]. Such differences lie in the physical thick- sheet. This is usually done by a pantographic or numerically con ness of the films and the methods of producing them. films were trolled system. The x-y coordinate table is moved by digital comThin arbitrarily defined as being less than 5 p (50 OO0 A) in thickness, mands and controls an engraving tool which cuts the appropriate for while thick films are greater than 5 p ; in fact, usually many times lines in a sheet of aluminum the mask. Photolithographic methods have been used to produce masks with perhaps the best resoluthicker than that. tion yet attained for stencils, the pattern is etched in very t i foils hn are Thick h generally produced by a direct physical applicaor tion, such as silk-screening and reflowing, whereas the films to be with resulting mechanical fragility. Likewise, glass ceramic masks The have been made by photoetching. prospect oflaser engraving of discussed in this paper are produced by more complex processes such as chemical vapor deposition, vacuum evaporation, sputtering, masks is interesting, but little has been reported concerning this etc. Although thick and thin films are often employed together, practice. Masks for high-resolution films can also be made by utilizing a the former will not be discussed inthis paper since they are treated mesh of closely spaced fine wires [5 11. This technique replaces the elsewhere. There are three general approaches the task ofpattern genera- single stencil mask by a combination of two masks: 1) a wire grill to tion in thin films. The first methodis analogous to the formation of a mounted close to the substrate and 2) an interchangeable metal photographic image; i.e., a f m of material is already present and mask mounted as close as possible to the wire grill. The gnll techi l nique is advantageous for depositing very fine patterns, particularly is exposed to a pattern of radiant energy which defines the corof a repetitive nature. responding image in the film. The image iseither latent or overt;if the former case, a development step, again analogous to photograPHOTOMASKING phy, is required. This direct generation method is only applicable to ratherspecializedinstances [MI. The secondmethod,which is Virtually al formation of high-resolution patterns is done by l much more widely applied, is the indirect generation of a film pat- photomasking and etching. This process uses a selective pattern tern. The most common form is the use of a photosensitive layer on called a photomaskto intercept certain portions and transmit other the film in which a pattern is desired. The photosensitive layer is portions of a beam of collimated light. The transmitted light causes exposed and developed, and then used as a protective mask while a chemical change in a photosensitive layer, called a photoresist etching away the exposed underlying material in a suitable etchant. on a surface closely adjacent the photomask. to A modification of the process utilizes some means of sensitizing a surface in the desired pattern, followed by selective growthdeposi- Photoresists or tion ofthe desired material only the pattern areas[49]. The final on There are many organic compounds whose structure and solupattern definition processuses a physical barrierto intercept selected bility change when exposed to light, pamcularly in the ultraviolet hs portions of a beam of material beforeit strikes and condenses on a regions. The h t materials foundto have ti property were natural surface. This method is often called stencil masking, and is most products such as gelatine, and organic colloids of this type have
x

IOw6R . a n

Remarks

~~

1396
LIGHT

PROCEEDINGS OF THE IEEE, OCTOBER 1971

ILLUMINATED =AREAS

PHOTDRESISl

t*\
RESIST: RESIST: POSITIVENEGATIVE RENDERED INSOLUBLE RENDERED SOLUBLE

SUBSTRATE

Fig. 3. General principles of positive and negative photoresists for pattern generation [41].

&3 c
ETCHED FILM PATTERNS:

0.wt
0.03t

0.02

I
1966

10.5

been used for some time to produce scales, reticules, and for other photoengraving application. In addition to being light-sensitive, a practical photoresist system must also have the ability to form ad1964 herent uniform coats which are not destroyed by the physical or are chemical action of the etching process. Lastly, selective solvents required to develop and finally remove the resist pattern. Generically, there are two types of photoresists. They differ in their response to light and their solubility. Materials which are rendered insoluble by illumination yield a negative pattern of the mask and are called negative photoresists. Conversely, positive photoresists become more soluble when subjected to light and yield a positive image of the m a s k . Both types of resist are utilized in practice and have their particular advantages and limitations, Fig. 3. Negative Photoresists: Commercially available negative photoresists, recommended diluting agents (thinners), and developers are in common use. Practical information concerning recipes and formulation is readily available and particularly abundantfor Kodak products [52]. The pMc@ constituents of a photoresist solution are a polymer, a sensitizer, and the solvent system. The polymers are characterized by unsaturated carbon bonds capable of reacting further and forming longer or crosslinked molecules.This reaction, however, must be stimulated by energy transferred by the sensitizer. The degree to which reaction and insolubility OCCUT depends on the exposureof the resist film. Polymerization of the resists while still in solution is neghgibly slow. Hence, resists stored may be in brown bottles for long periods of time. Small amounts of antioxidant compounds to m e r stabilizethesolutions and surfactants toenhance wetting of the substrate surface are sometimes added. Positive Photoresists: So far, there seems to be only a limited group of commercially available positive photoresists, and these products are discussed in the literature [41]. O the resists listed, f AZ-1350 is the most suitable for h e line etching. Others, e.g., A Z - 3 4 0 , are chemically similarbut have a higher solidscontent and yield thickercoats as required for deep etching and photoengraving. The low viscosity of AZ-1350 indicates a relatively low molecular weight (211OOO) of the resin. The solubility of the resin, after evaporation of the solvent, is strongly dependent on the functional groups present in the macromoldes. These groups are responsible

0.01 1962 (960

1974 1972 1970 1961(

YEAR

Fig. 4. Typical metal-6lm linewidth capability as a function of time (1961-1971).

for .the initial insolubility of the resin in the developer which is an aqueous buffered sodiui~ hydroxide solution. When the resistl is m l i illuminated, the sensitizer transfers energy to the functional groups of the polymer which thereupon change and render the resist film soluble. The solubility is MKOW~Y confined to the immediate vicinity of the absorbing chromophores. Therefore, positive resists yield good resolution even in relatively thick For example, 5 p wide coats. lines can be developed in 6 p thick layer.
Photoresist Pattern Formation Application and processing of photoresist films is a highly empirical art. The procedures vary in detail fromplace to place. Thus when a photoresist processing facilityestablished, it is necessary to is adjust the conditions and process parameters until a stable procedure is reached. Removal of Photoresist

The f d removal of cross-linked polymer films is an onerous task because these compounds are not truly soluble. The degree of difEculty encountered depends on the nature the photoresist film, of its thickness, and the underlying substrate. In general, stripping resist films becomes more difEcult the higher the post-baking temperature. The most widely used resist removal techniques rely on hot chlorinated hydrocarbons to swell the polymer in conjunction with acids to l o o s e n the adhesion of the resistfilm to its base. Oxidizing agents, likehot H,SO,, may be used to decompose the organic material, but film corrosion often prohibits such drastic action. Subsequent swabbing or brushing operations are nearly always necessary to remove tenaxiously clinging fibers or patches of the resist at the risk of mechanically damaging the film pattern. The jet action of spray rinses is generally not completely satisfactory, so a second rinse, a common practice, washes away the loosened resist shreds i n

GREGOR : THIN-FILM PROCESSES FOR MICROELECTROMCS

1397
INTERMEDIATE TRANSPARENCY (1O:ll MASTER 11:l) WORKING SUBMASTERS MASKS

ARTWORK 1200.1)

LIGHT

___)

7 l
120x1

i /
REPEAT

P R I- T IC O NR E D U C T I O N 2 N D R E D U C T I O N N vG T A C T N 1ST (10x1

- I/

Fig. 5.

General method of fabrication of photomasks [41].

tically and printed out to the final size on a master photomask, and a Fig. 5. To achieve the maximum accuracy resolution of the h l photomask (which earlier was seen to be -0.oooO5 in), great care must be taken insure that the to original layout is as sharp as possible. Instead of drawing the pattern, it cut from a material offering high is contrast and attached to a base. The base material is a polyester iilm such as Mylar, while a variety of pattern materials have been used such as Rubylith and Studnite [41]. This master image ( x 10) Resolution of Photoresists is then reduced and projected onto special emulsioncoated glass The question of ultimate resolution attainable with the present resists is of great concern in integrated technology. The circuit speed plates which are optically flat surfaces and free of defects either in and density of these circuits may ultimately be limited by size- the emulsion or the glass. Since the working image is much smaller imposed restrictions in the photoresist technology. The problem of than thesemiconductor area on which it will be projected,the resolution involves several factors. A single bridging between two method used producesan arrayof multiple images( x 1) ofthe patclose-spaced lines caused by a particle of foreign matter in the film tern. Using one method, a special camera projects the image onto (or may be interpreted as a resolution problem, whereas, actually, the the emulsion. Then the emulsion is moved stepped) a certain distance, and the projection repeated. This method is thus called true resolution capability of the resist has not been approached. a specialmultilens It appears that the ultimate resolution of the present resists will step-and-repeat.Anothermethodinvolves projection system which simultaneously projects separate images never be achieved in any practical application. Lines 0.0o01 wide in separated by O.OOO1-in spaces are possible with present techniques. from a single source. This is referred to as the flys-eye method, The resist must be carefully filtered and meticulous cleanliness ob- because of the resemblanceof the multiple lensto that of the comserved. This assumes that a uniform resist film 0.0001-0.0002 in pound eye of the fly [54]. The conventional technology of masks is expensive since the thick can be applied,and relates only to shortlines. The decrease in wear occurring when the mask touches the photoresist surface reminimum practicable linewidth for integrated circuits during the quires frequent replacement. Also, the numerous small errors and past decade is shownin Fig. 4. occur The material to be etched away should, in general, not exceed random dimensional changes which during the complex maska the resistfilm thickness, if resolution isto be determinedby the film. making process generally cause particular mask to align properly only with others of its own particular set. Finally, the drafting and For deep etching, the amount of undercut by the etchant must be cutting operations are slow and difficult to check for error.A numtaken into account and compensated for in the dimensions of the to mitigate these problems. two image. Of the general photoresisttypes commercially available, ber of recent developments have sought By using a thin film of chromium on a glass blank, the pattern the positive substances seem to possess higher resolution and are can be transferred via conventional not as sensitive to fogging by oxygen from the atmosphere. How- of a master emulsion mask photomask operations to the much more durable chromium film ever, negative resists may offer somewhatbetter adhesion to under[SI. Also, the edge acutance of the chromium pattern is better. lying surfaces. Another method for extending mask life isto coatthe emulsionsurFabrication of Photomasks face with a protective layer of transparent material as SiO, or a such General: The production of photomasks begins with original polymer film. the pattern layout several hundred times larger than the fnl pattern. ia Light Beam Mask Fabrication: The development of automatic A specialcameraisemployed to produceasmallerimage of pattern generation equipment allows a focused beam of light to the pattern on a photographic plate, usually to 10 times the final expose the master emulsion selectively. Selectivity is achieved by the programming the motion of the emulsion plate under light beam size. This reduced master image is then once again reduced opa forced stream of water solvent. Some success has been achieved or in nonliquid resist removal. Highly reactive media (ozone, 0,free radicals, and plasmas) can convert the organic photoresist to CO, and H 2 0 [53]. Elevated temperatures (- 200C) are required, and the plasma environments may detrimental to devices sensitiveto be surfacecharges,such as MOS circuitry and high-voltage diode arrays.

1398

PROCEEDINGS OF THE IEEE, OCTOBER

197 1

and a shutter. The program is generated by using the appropriate language to translate a wiring diagram into an interconnection pattern by combining logical layout rules with dimensional or geometric rules. Error checking and generation of copies is accomplished morereadily and quickly, and modification are rapidly transformed into working photomasks [56]. Electron beams offer an order of magnitude increase in resolution. Furthermore, the high energy density and ease of beam deflection make production of patterns by tracing with a deflectable the beam seem potentiallyrapid. However, a beam of charged particles q i san elaboratesystem for guidance and control. u r e Considerable study of direct exposure of resistfilms by electron beams has led to p r e m usage of t i method. High resolution hs can be achievedas well as high pattern formation rates. The earliest attempts using direct electron exposure employed fixedb a s but e m, more recently sophisticatedbeamdeflection methods have been devised [57]. With this method, linewidths of p are readily achieved, l and spot diameters of 100 A are attainable. A variation of direct pattern generationemploys a beamofconsiderableenergy to film,the remainingfilm functioning as a positive volatilize the resist resist. This method is applicable to forming holes in the resistfilm for subsequent etching of holes, formation of vias,etc. via A rapidexposure process using electron bombardment has been reported [58]. An image of the pattern is produced by secondary electron emission from the mask image, with accelerating potenan tial to direct the emitted electrons to the wafer surface. The electron beam is thus analogous to ultraviolet light and the entire surface is not exposed in a very short time. Since image reduction is easy, the process requires as careful mask making as in conventional photolithography. Recently, there has considerable interest in hologbeen raphy due to the rapid development of laser optics. Since no lenses are involved, off-axisaberrations are problem. Furthermore, deno fects in holograms are not the transmitted along with the image [59].
Maskless Pattern Formation

1WO WATT MERCURY

BEAM SPLITTER FILM PLANE (1.25 DIAMETER SILICON WAFER1

-- - \ _

e
_ / - - -

I
1
PH~TOGRAPHIC MASK OF PATTERN

I
1
OSTAPKAR

\LENS

UOal

I
I

I
1
I

CONDENSER

I
I
I

I I I

VIEWING SCREEN

Fig. 6. Formation of patterns by direct projection of image onto surface. Shown i a x 10 reduction of pattern onto a w f r s ae.

2) The etchant must selectively attack the thin film and not the photoresist or surfaces under the thin film. 3) Formation of gas bubbles is highly undesirable.

Contact photomasking has certain difficulties associated with practical use, such as unwanted mask defects, transfer of material by contact, wear of the emulsion, and resolution limits due to diffraction. Many of thesecan be overcome in principle eliminating by the mask and directly exposingthe resist film. This can be done by projecting an image of the desired pattern onto the film using a focused spot of lightor beam of electrons to trace out the pattern, or using irradiation to promote a chemical reaction and deposit or remove material [a]. Projection ofan optical image requires optical system such an of perfection that t i process has yet been widely adapted. Theprinhs cipal problems are the difficultyof maintaining a flat focal plane for the image over large areas, and the alignment of two or more patterns. The ultimate limit of resolutionis imposed by the diffraction of light, hence this method does not offer a large potential for increased resolution over contact masking. A direct process lens reduction scheme is shown in Fig. 6.

A list of common etchants for thin films was given previously in Table IV. The most widely used etchants are bufered aqueous solutions of HF, specrfic for SiO, and silicate glass m, which do not attack or swell photoresist films and generate no troublesome gas bubbles. For metal films, various mineral acid solutions can be employed if the metal is not reactive. Noble metals suchas PI and Au require complexing-type chemical reagents etching. for Some substances are difficult to etch by conventional methods, and special techniques have been devised. Silicon nitride is an example; it is difficultto etch Si,N, with buffered HF because the low etch rate results in photoresist deterioration before the process is completed. However, has been found that hot it concentrated H3W4 etches Si3N, much faster than SiO,. Hence, a layer of CVD SiO, is depositedon Si,N,, standard photoresist used to develop the pattern in the SiO,,and the hot H,W, then etchesout the Si,N, [61]. Sputtered Bi,03 is a convenient etch resist film which can be deposited as low temperatures [62].
Reverse Photolithography

Thin films of substances diilicult to etch may patterned by use be of reversephotolithography which isoften referred to as liftoff or stud etching [63]. In this procedure, a base film is deposited and formed into a pattern which is the obverse of the one desired. Then the desired material is deposited over the base film and surface. im Treatment in a medium which attacks the base fl but not the overlying film produces the desired pattern. Among the substances used for the base film have been Al, KPR, MgC1,. The process fl is several times thicker than the im works best when the base n overlying film. A schematic illustration of the process is shown i Fig. 7. Subtractive Etching An extension ofthis method, using electron bombardment, has A wide variety of etchant solutions have been used to subtrac- recently been employed to etch patterns in silicon oxide layers for tively etch metals, dielectrics, and other t i fl materials. The planar transistor fabrication. The etch rate of the bombarded film h n im choice of etchant depends on the nature of the system usedto bring was 2-3 times faster than theuntouchedregions [&I. Electron a the etchant and film together. In general, the etchsolution is either, bombardment must be done under conditions which do not form polymerized pumpoil layer on the surface, for electron-beam polystirred or agitated so as to continuously bring fresh reagent incontact with thefilm. Alternatively, spray etching be used; the pur- merized 6lms can act as a resist to etching [65]. can pose is to maintain a constant concentration of reagent and hence a Sputter Etching constant rate of etching. Beeause of several necessaryor highly deCertain materials are difiicult to etch with conventional chemical sirable restrictions, the actual number ofsuitable etchants is reduced reagents. This is due to their extreme inertness (sin the case of a greatly. In general, theseconditions are as follows. siliconnitride or cermet films) or because of the variability of etching fairly be rapid. behavior (siliconnitride, silicon monoxide). Recently, the process of 1) The etch rate must

GREGOR: THIN-FILM PROCESSES FOR MICROELECTRONICS


NEGATIVE , RELIEF MASK SUBSTRATE ,

1399

/
S

DEPOSITED FILM

ing impurities from the Si. In particular, those fast-diffusing impurities which decreasecarrier lifetime in bulkSi can diffuse to and be trapped in the SiO, layer [68]. The backside of the Si wafer is the most likely place where gettering occurs. Thin films of organic photoresistare ubiquitous in pattern generation, but other materials are occasionally employed etch resists. as As mentioned earlier, SiO, films are useful as resists for etching Si3N4 with hot H3P04 [61]. Films of chromium-silver have been shown to resist concentrated HF solutions, allowing Si3N4 to be etched rapidly[69]. Occasionally, thinfilms perform bothas process aids and as functional elements of the device. An outstanding example is the use of polycrystalline silicon in the silicon-gate MOS device [I I]. The silicon film is usedas thediffusion maskso that the source-drain spacing is automatically aligned to the gate electrode. Afterwards, the silicon functions as the gate electrode in circuit operation. Likewise, filmsof Si02 are useful in allowing the method of dielectric isolation to be employedincomplementary circuit fabrication.

APPLICATIONS DEVICE Most of the important phenomena govern the function of a that microcircuit or device are embodied in thin films. On the device sputter etchingor subtractive removal of material ion bombardby isulation, ment hasbeen developed [66]. The method dependson the fact that level, the functions of surface passivation, connections, most materials have lowenergy sputtering yields thatare approx- terminals, and environmental protection are performed by films of imately the same. Hence, a photoresist film and another film will metal, glass, S O z , etc. From a circuit standpoint, the introduction both erode by positive ion bombardment at about the same rate. If of resistance, capacitance, voltage and current paths, interconnecthe the photoresist isthicker, it will still be present after the underlying tions, and terminal points involve use of thinfilms. The stability film is completely removed. The advantages of this etching method and reliability of the component in use are largely dependent on films in its structure. are its generality and independence of material properties, its faith- the properties of the thin The passivation of the surface of a semiconductor is a complex ful reproduction of the resist pattern, and its cleanliness. Disadproblem. In chemical usage, the term passivation conventionally vantages are the necessity for vacuum and RF equipment, batch are : processing (limited quantity), and straight f m pattern edges. The refers to the process of rendering a surface unreactive. Examples i l iron in concentrated acid and aluminum in contact with the atfilm. Due latter often causes problems with subsequently deposited mosphere. Thus the process involves the formation of aon the layer to the phenomenon of resputtering, some of the removed film will inhibits further chemicalreaction. In the case semiof find its way back to the surface unless a catcher is usedretain the surface which to conductors, not only chemical also electrical stability is required but sputtered material [67]. for a passivated surface. Hence semiconductor surface passivation means electrical as well as chemical stabilization. h m APPLICATIONS It is appropriate todivide the passivation of semiconductor surThe fabrication process most silicon for and other semiconductor faces into two major categories. First, in primary passivation, the on microelectronic devices is based the production of precisely de- objective is the control and stabilization of the semiconductor surfined areas of controlled dopant concentration in the surface region face electrical properties. Then there is the secondary passivation of the semiconductor. Modem microcircuits would not be possible which may be thought of as the protection or stabilization of the without the ability to dope selectively to a resolution whose precision primary passivating medium. The secondary passivation method is measured in microns. This is possible because alarge number of also performs the functions of insulating and protecting the interdopant atoms are blocked from diffusing into the semiconductor by connection and terminal metallurgy as well as providing overall protection. Secondary passivation is a thin of SiO,, Si3N,, etc. The unique combination of properties mechanical and chemical film of SiO,t i films have made LSI possible. These simultaneous normally provided by some form of thin-film overlay, although the hn are its ability to electrically passivate silicon to block diffusion of boron, earlier practice of bonding the unprotected chip and hermetically phosphorus, and arsenic, and to be etched selectively by buffered sealing the unit in a container is still widely practiced. For MOS circuits, which are more sensitive to stray charge on the oxide surH F solutions. Thin films of SiO, are also capable of shielding underdielectric layer over the lying substances from ion penetration, depending on the energy of face, deposition of some form of protective as attested the ion. Thus the doping of semiconductorscan be carriedout using metallurgy and the thermal SiO, is highly recommended, ion beams to implant the desired dopants and SiO, to act as the by numerous manufacturers [70]. The most popular methods are CVD or sputtered SiO, for integrated circuits, and fused glass for mask [57]. discrete components. Among more recent candidates for this purThe source of dopant atoms for diffusion into the surface is pose are silicate glasses containing phosphorus, aluminum, lead, usually from a layer deposited from some ambient gas. However, the sourcecan be a liquid suspension coatedon the surfaceand then silicon nitride, or poly-pxylylene. It should be noted that plastic converted to a solid film at elevated temperatures. This method, encapsulation, in which thecircuit or component chipis sealed into requires a reliable secondary called paint-on diffusion, was discussed earlier as an example of a molded polymer package, generally physical deposition of films [26]. This method maybe useful in passivation method as well as the plastic package. thin The use of deposited Si02 is neceSSary for MOS integrated cirsimultaneous formation of p and n-channel FET devices in comcuits for a reason beyond those mentioned. passivation makes SiO, plementary MOS circuits. causes inThin films of SiO,are often grown Si with the on intent of getter- the circuit less sensitive to surface charge migration which

Fig. 7.

Method of film etching known as lift off [41].

1400

-v > v T
IF

PROCEEDINGS OF THE EEE. OCTOBER

1971

-a

IS L A R G E OR

IS SMALL

\ \ \ \ \ \ \ \ \ \ . E! \ \ \ \ \ \ \

P+

Pt

FOR SAME -R VT LARGE BECAUSE X IS LARGE

Fig. 8. Cross section of silicon integrated circuit illustratingeffect of charge - Q on insulating film surface. Silicon surface inversion caused by - Q (top) is prevented by interposing a sufiiciently thick dielectric layer between - Q and silicon (bottom).

relativelymassive extensions of the interconnection metallurgy suitable for welding to chip carriers orlead frames. Beam leads are usually formed by electroplating a relatively heavy deposit of a metal,suchasgold, on the thin film interconnections. Another method is the solder reflow fabrication of terminal bumps by allowing a fusible thin-film deposit such as Sn-Pb to flow into and form a pad on a previously deposited terminal area, such as Cr-CuAu. The solder bump is then h e to the appropriateconnections sd on a substrate [74]. Because of their small size and sensitivity, certainthin films have found special applications as photosensitive, heat sensitive, and strain sensitive devices. The most common are photoconductive films such as CdS and CdSe [75]. Thin-film thermometers which measuremaximum temperature have been made fromCr-SiO, exploiting these films temperature coefficient of resistance [76]. The use of read-only memories fabricated from MOS circuit arrays has been stimulated by the development ofprogrammable ROM arrays (PROM). Unlike the earlier custom devices made by specially programmed interconnection patterns applied to a standard array, the latter consist of arrays in which s ele address locations can be pcid f permanentaly denoted by disconnecting a l n at this point. This is ik usualIy done by applying a currentpulse to open a fusible thin-film metallic connection.

version of the underlying high-resistivity silicon,see Fig. 8. Although CVD methods are more popular, it has recently been shown that sputtered SiO, also can be used for this purpose [72]. Fortunately, thin layers of SiOl are also excellent insulators, and furnish the insulation between the semiconductor and the metal films used for contacts, gateelectrodes, and interconnections. By usingSiO,, capacitance can also beintrodwed on the semiconductor, although limited to small values by the relatively low dielectric constant of SiOt and the small electrode areas afforded. The formation of electrical contacts to the semiconductor is achieved by etching via holes at the appropriate places in the oxide layer and depositing a metallic layer which makes a low-resistance contact at the via hole. Subsequently, an interconnection pattern is etched in the metal film. For complex highdensity bipolar integrated circuits, a second or third layer of metallization is usually necessary to allow complete wiring of the circuits which requires an additional insulating layer, generally SiO,. The most common metal used is aluminum, pure or alloyed with soluble metals. Based the on usual criteria of low contact resistance, high conductivity, ease of etching, and chemical stability, aluminum is easily the best choice. However, there are certain disadvantages such as mechanical softness, relatively low Al-Si eutectic temperature (577C), and low current-density limit, which have stimulated the development of other metallurgies, such as Cr-Ag,Mo-Au, Pt, and Ti. A comparison of the important features of these metal films is given in Table N. Although polycrystalline Si would normally be considered a not possible material for thin-film interconnections, thinflsof Sihave im found use in a related area, the gate electrode material for MOS integrated circuits. Since is also employedas part of the diffusionit masking step, the can not be used for contacts to Si source and drain regions. However, it be used in can certain ways to assist in the interconnection task, and can also be used as a guard plane to protect against surface inversion [73]. Molybdenum films have been employed in similar fabrication schemes [74]. Terminals for microelectronicdevices and circuits are often made by thin-6lm methods. The simplest method merely extends the terminus of an interconnection line to a su5ciently large area to allow wire bonding by ultrasonic or thennocompression methods. More sophisticated techniques involve the formation of beam leads,

FUTUREDEVELOPMEKIS
The futurecourse of thin-film technology developmentappears to be in three major directions: the improvement and expansion of present capabilities, the exploitationof novel thin-film phenomena for electronic use, and the establishment of pure thin-filni electronics. These are not completely independent and overlap to some extent. Also, the past decade has shown that technology forecasting not a is completely accurate science. In the area of thin films, the considerable potential growth predicted for cryoelectronics failed to materialize, while the capabilities of MOS LSI were scarcely dreamed of. Bearingthis in mind, a brief discussion of theseareas of develop ment will be given. Expansion and Improvemen1 The understanding of some of basic h nfilm deposition meththe ti ods is well-founded (vacuum evaporation, anodization) but other methods are justbeginning to become unitied in terms of models to understand the present and predict future behavior. In particular, sputtering and chemical vapor deposition seem to have significant untapped areas as far as better control of film properties, more flexible deposition rates, and upscaling of production capability are concerned. It now appears possible to produce a rich variety of chemical compounds and mixtures of thin films by either method, with sputtering being the more diversified, since it not restricted to is materials resulting from thermodynamicallyfeasible reactions. Likewise, by usingtargets of mixed composition, a vast number of films can be produced whose properties can be altered subtly by varying the method of deposition. The extension of surface passivation by thin films from silicon to othersemiconductors is another areawhere improvement can be expected. Inparticular,the reliability and lifetime electroof luminescent diodes fabricated from GaAsP and other 111-V semiconductors should be increased through better understanding of surface passivation. High performance devices may also possible be in these high-mobility materials, if planar methods of fabrication can be extended successfully from silicon. In silicon, better understanding of the natureof thin oxide films can be expected, along with improvements in metal films, photoprocessing, etc., to push the size of integrated circuitsto adensity of 4-8 times greater than achieved at present. In particular, theinter-

GREGOR THM-FILM PROCESSES FOR MICROELECTRONICS

1401

action of the various thin-film processes with each other will be and a receiver electrode. It uses a novel concept for controlling the sufficientlyuntangled to allowdynamic and regenerativemultitransfer of electrical charges across the surface of a semiconductor phase circuit designs to be implemented in nchannel MOS tech- [8 1 1. Fabrication of the device begins with a silicon surface covered nology. Likewise, the further development of high-speed Schottky- with a layer of insulating film10oO A thick. The source and receiver barrier MOSFET devices can be expected to progress as rapidly electrodes-separated by a narrow slit-are formed by depositing as metal-silicon barrier technology and projection photoprocessing a layer of refractory metal, such molybdenum, over the as insulating advance [78]. electrodes,and film. A second insulating film is deposited over these The demands for metallurgy capableof handling highercurrent the third narrow electrode-the transfer gate-is then deposited so densities than aluminum will probably continue, but is difficultto that it overlaps the thin slit between the source and the receiver it forecast any breakthroughs in area, since almost all the likely electrodes. The transfer gate controls the transfer of charges bethis of metals and alloys have already received sufficient attention tobring tween the source (higher level) receiver (lower level) and electrodes. out their merits and weaknesses. For bipolar integrated circuits, Only a small amount of charge on thegate is required to control the transfer of a much larger charge across the gap between the elecand Ti will probably find increased usage. thin films as Cr, Ag, Recent developments in the technology of substrates for trodes. As a result, the device has both charge and voltage gains. suitable heteroepitaxial deposition of Si films may open up an era of SOS The Josephson effect refers to the tunneling across a thin dielec(silicon-on-substrate)integrated circuits. Both sapphire and spinel tric film of paired electrons from one superconducting film to ansubstrates appear suitable, with the latter material becoming more other [82]. Most of the experimental studieshave been performed on of an popular. The excellent isolation and minimizedjunction capacitance Pb films on which a film PbO about 20A is grown. The device is of SOS bipolar circuits, as well as compatibility of the MOS device extremely sensitive detector has highly nonlinear characteristics. and technology and the transparency of the substrates, may allow the Many possible applications have been discussed, and undoubtedly formation ofhighlycomplexmixedarraysofsiliconswitching, others will be developed as the experimental techniques are improved. Since the film superconducting, a cryogenic environment is storage, and driver circuits with various kinds of optoelectronic on (liquid helium) is required. A tunneling cryoton based a Josephfunctions. been studiedfor use as a possible switching element With increased understanding and controlof thin-film process- son junction has ing, it will be feasibleto combine themore advantageous features of for logic applications [83]. A simple devicefor storing information in a circulating fashion several device technologies into complex circuits and subsystems. forFor instance, the combination ofMOS and bipolar transistors on a has recently been investigated. The principle of operation is the monolithic silicon die combines the packing density and high im- mation of a depletion layer in high-resistivity at the surface by silicon pedance of the former withthe high-performance surge protection applying a voltage a t i film on the oxide surface [84]. By using to h n use of thelatter. Another example is the of Schottky-barrier diodes appropriately shaped electrode patterns and/or multiphase voltage in FET circuits to increase speed; the itself may a Schottky- pulses, the depletion layer charge can be shifted serially. Sensing of FET use barrier gate [77]. or the capacitance of theMOS dot determines if the charge is is not present. The device hasas its major advantagethe simplicity ofconNovel Phenomena struction. Since the depletion layer can be altered by photo-geneA number of effects involving thin films investigationhold rated electron-hole pairs, the device has some possible applications under some promise for future applications. The variable-threshold FET in photodetection. Other potential uses are in shift registers. device isan outgrowth of the work Si,N, films for passivation of on The phenomenon mentioned previously sometimes referred is to oxidized Si and other whiconductorsurfaces. It was observed that as an electrostatic bubble because of its partial analogy to the to relativelyhigh whenSi3N,-Si02sandwichesweresubjected widely publicized magnetic bubble or domain formation which voltages in MIS structures, the flatband voltage could be shifted occurs in certain materials [85]. The best known are orthofenites considerably.Theseobservationsled to themetal-nitride-oxideand garnets. These are fabricated in the form of platelets carefully silicon (MNOS) FET, whose threshold voltage can be reversibly cut so that the easyaxis is perpendicular to the plate. Upon applying shifted by applying a voltage pulse. The potential applicationsare in a magnetic field, circular domains 0.0024.005 in in diameter are high density storage bit/device), electronicallyset ROM, and (1 non- formed. By using appropriately shaped thin fl electrodes, called im volatile storage. At present, the most efficient form of the device t-bars, the domain can be propagated from one spot to another requires that the SiOz thickness be thin enoughefficient tunnel- [86]. for Sensing can done by u e of the Faraday be s effect, which renders ing of electrons, -21A. Considerable fundamental and applied the domains visible with polarized light. Many applications suchas development are still needed to understand the process of charge shift registers, circulating storage, logical functionsof binary multiretention and to establish values for reproducibility and reliability. plication and division, etc., have been demonstrated. Another class of device receiving much notice is the variableresistance or bistable thin-film diode. This deviceconsists of a thin Pure Thin-FilmElectronics film of a material between two electrode films with a high dc imFor many years, efforts havebeen made to develop an electronic pedance whichdrops rapidly at some voltage and remains low until component or circuit based entirely on thin films. The chief benefits the voltage polarity is reversed. The most popular materials have been amorphous semiconducting chalcogenideglass films prepared of such an approach would be lowcost fabrication plus certain by vacuum evaporation[78]. Considerable workhas been done with exotic features for specific technologies. In the past, a number of Nb,O, films produced by anodization [79]. Relatively high switch- devices were considered, but no serious contender to the semiconare ing voltages are required and much is still unknown about the de- ductor single crystal exists today. Some of these wayside devices tailed mechanism of the transition or its consequences to device listed in Table VI. There do not appear to be any thin-film devices reliability and lifetime. Adifferent type of bistable behavior is mani- which are likely to supplant the present monolithic technology, but fested by certain thin organic polymerfilms. In this case, the device some interesting developments are possible. The bistable switching can be read at low voltages to determine its previous history [SO]. element described in the previous section is a pure thin-film device are A new semiconductor device called a surfacecharge transistor as made today. Likewise, Josephson-effect junctions made from hn no is a circuit element with three electrodes-a source, a transfer gate, t i films. These two classes of device, however, exhibit gain or

1402

PROCEEDINGS OF THE IEEE. OCTOBER

1971

TABLE VI THIN-FILM ACTIVE DEVICFS


~~

Device Space-charge limited triode High-field triode Hot-electron triode Metal-base transistor Tunnel-emission triode Thin-lilm field effect transistor Superconducting In-line cryotron Crossed-6lm cryotron Resonistor

Remarks lack of suitable material nonreproducible nonreproducible tunnelling difficult to control low carrier mobility; instability low temperature required; complicated interface low gain and performance complex structure

require an exotic environment. A general-purpose thin-film active device does not yet seem to be available. Thin-film transistors of various sortsare still being studied; recently it was reported that TFT devices using selenium the semiconductor have as been fabricated on flexible plastic fl substrates by an inexpensive batch fabrication im process 1871. However, the use of such devices wouldappear to be limited to low-performance applications. The limiting cost baseof electronic functionswill probably turn out in the future to be the silicon wafer itself. When that point is reached, and if the basic understanding of thin films continues to broaden and deepen, there may once again be intensive activity in the study of hotelectron triodes, metal-base transistors, TFT devices, etc. Phenomenasuch as electrochromic films, polymer tunneling barriers, or high-temperature superconductors may lead to devices as yet only dimly perceived. The potential for extremely low costand wide applicability still exists.
REFERENCES L. Holland, Ed., Thin Film Microelectronics: The Preparation and Properties of Componentsand Circuit Arrays. New York: Wiley, 1965. L. V. Gregor, Passivation of semiconductor surfaces, Solid State Technol., Apr. 1971, pp. 37-43. P. Balk, C. F. Aliotta, and L. V. Gregor, Microstructural properties of thermally grown SiO, layers, Trans.Metall. SOC.AIME, vol.233, 1965, p. 563. B. E. Deal and A. S. Grove, General relationship for the thermal oxidation of silicon, f . Appl. Phys., vol. 36, 1965, p. 3770. L.Young, Anodic Oxide Films. London, New York: Academic Press, 1961. P. F. Schmidt and D. R. Wonsidler, Conversion of silicon nitride films to anodic SiO,, f . Electrochem. SOC., 114,1967, p. 603. vol. P.W. Anderson and J. M. Rowell, Probable observation of the Josephson superconducting tunneling effect, Phys. Rev. Lett.,vol. 10, 1963, p. 230. E. C. Ross and J. T. Wallmark, Theory of the switching behavior of MIS transistors, RCA Reo., vol. 30, 1969, p. 366. A. Waxman and K. H. Zaininger, Al,O,-silicon insulated gate field effect transistors, Appl. Phys. Lett., vol. 12, 1968, p. 109. RCA Rev. (Special Issue on Chemical Vapor Deposition of Conducting, Insulating, and Semiconductor Films), vol. 12, Dec. 1970. J. C. Sarace, R. E. Kenvin, D. L. Klein, and A. Edwards, Metalnitride+midejilicon FETwith self-aligned gate, Solid-state Electron., vol. 11, 1968, p. 653. T. L. Chu, Dielectric materials in semiconductor devices, 1. Vac. Sci. Tech., vol. 6, 1970, p. 25. E. J. Mehalchick and M. B. MacInnis, Preparation ofvapordeposited Tungsten at atmospheric pressure, Electrochem. Technol.,vol. 6,1968, p. 66. H. F. Sterling and R. C. G. Swann, Chemical vapor deposition promoted by RF discharge, Solid-State Electron., vol. 8, 1965, p. 653. L. Holland, Vacuum Deposition of Thin Films. London, England: Chapman & Hall, 1963. E. H. Snow and A. S. Grove, Radiation study on MOS structures, Contract AF 19(628)-5747, Rep. 1, Air Force Cambridge Res. Labs., June 1966. o& L. Braun and D. E. L o Precision thin-film cermet resistors for integrated circuits, Proc. IEEE, vol. 54, Nov. 1966, pp. 1521-1527. G. K. Wehner, Advan. Electron. Electron. Phys., vol. 7, 1955, p. 239. P. Davidse and L. I. Maissel, Dieletric thin film through RF sputtering, 1. Appl. Phys., vol. 37, 1966, p. 574.

[20] R. Frank and W. Moberg, Preparation and properties of reactively sputtered silicon oxynitride, f . Electrochem. SOC., vol. 117, 1970, p. 524. [21] L. I. Maissel, R. E. Jones, and C. L. Standley, Re-emissionof sputtered SiO, during growth and its relation to 6lm quality, IBM J . Res. Deoelop., vol. 14, 1970, p. 176. [22] G. C. Schwartz and R. E. Jones, Argon content of SiO,filmsdeposited by RF sputtering in argon, IBMJ. Res. Develop., vol. 14,1970, p. 52. [23] J. S. Logan, Control of RF sputtered 6lm properties through substrate tuning, IBMJ. Res.Deoelop., vol. 14, 1970, p. 172. [24] E. M. Davis, W. E. Harding, R. S. Schwartz, and J. J. Corning, Solid logic technology: Versatile, high-performance microelectronics, IBM f . Res. Develop., vol. 8, 1964, p. 102. [25] E. F. Platz, Solid logic technology computer circuits-Billion hour reliability data, Microelectron. Reliability, vol. 8, 1969, p. 55. [26] Emulsitone Company, Livingston, N. J., company publication. [27] R. M. Handy and L. C. Scala, Electrical and structural properties of Langmuir films, f . Electrochem. SOC.,vol. 113, 1966, p. 109. W. H. Simpson and P. J. Reucroft, Quantum-mechanical tunneling in thin films of chlorophyll-a, Thin Solid Films, vol. 6, 1970, p. 167. L. V. Gregor, Polymer dielectric films, I B M f . Res. Deoelop., vol. 12, 1968, p. 140. W. F. Gorham, A new general synthetic method for the preparation of linear poly-p-xylylenes, f . Polymer Sci., vol. 4, 1966, p. 3027. S. M. Lee, J. J. Licari, and I. Litant, Electrical reliability of Parylene lilms for device passivation, Metall. Trans., vol. 1, 1970, p. 702. L. N. Alexandrov, E. I. Dagman, V. I. Zelevinskaya, E. I. Patrosjan, and P. A.Skirpkina, Peculiarities of formation and properties of semiconductor films deposited by electrical explosion, Thin Solid Films, vol. 5, 1970, p. 1. J. M. Nobbs and F. C. Gillespie, Properties of thin films of ZnO prepared by a chemical spray method, 1. Phys. Chem. Solids, vol. 31, 1970, p. 2353. W. A. Pliskin and R. P.Esch, Refractive index of SiO,6 l m s grown on silicon, f . Appl. Phys., vol. 36, 1965, p. 201 1. M. Hacskaylo, Refractive index of thin dielectric films, f . Opt. Soc. Am., vol. 54, 1964, p. 198. N. Hamck,Internal Reflection Spectroscopy. New York: Interscience, 1967. L. V. Gregor, Study of silicon nitride as a dielectricmaterial for microelectronic applications, Air Force Avionics Lab., Wright-Patterson AFB, Dayton, Ohio, Tech. Rep. AFAL-TR-68-272, Nov. 1968. C. A. Mead, High field current flow processes in insulating films, thin presented at Electrochem. Soc. Meet., Los Angeles, May 11, 1970. M. H. Monnier, Trimming t i 6lm resistors by direct resistance hn heatings, IEEE Trans. Parts, Mater.,P a c h g . (Corresp.), vol. PMP-2, Mar. 1966, pp. 44-45. A. Y. C. Yu, Electron tunneling and contact resistance of metal-silicon act barriers, Solid-State Electron., vol. 13, 1970, p. 239. [41] L. I. Maissel and R. Glann, Eds., Handbook of Thin Film Technolozy. -. New York: McGraw-Hill; 1970, ch. 7. W. A. Pliskin, The evaluation of thin film insulator, Thin Solid Films, vol. 2, 1968, p. 1. E. Yon, W. H. KO, and A. B. Kuper, Sodium distribution in thermal oxide on silicon by radiochemical and MOS analysis, IEEE Trans. Electron Deoices, vol. ED-13, Feb. 1966, pp. 276-280. P. J. Burkhardt, Tracer evaluation of hydrogen in steam-grown SiO, lilms, f . Electrochem. SOC., vol. 114, 1967, p. 196. C.L. Standley, R. E. Jones, and L. I. Maissel, Sputtered SiO, deposited over a step, Thin SolidFilms, vol. 5, 1970, p. 355. I. A. Blech, Evaporated 6lm profiles over steps in substrates, Thin Solid Films, vol. 6, 1970, p. 113. R. E. Thun, J. A. Ciccio, D. E. Greentham, R. W. Ilgenfritz, M. P. Lepie, and S. M. Stuhlbarg, Printed and molded circuits; integrated microcircuits, InsulationlCircuitry, vol. 16, 1970, p. 250. L. N. Kaplan, Photoetching of Pb films with nitromethane, f . Phys. Chem., vol. 68, 1964, p. H. L. Caswell and Y. Budo, Formation of thin film circuits using preferential nucleation, Solid-State Electron., vol. 8, 1965, p. 479. J. W. Bremer, Superconductive Devices. New York: McGraw-Hill, 1962. P.K.Weimer, The TFT-A new thin-6lm transistor, Proc. IRE,vol. 50, June 1962, pp. 1462-1469. Applications Data for KO& Photosensitive Resists. Eastman Kodak Co., Rochester, N. Y., pamphlet, Dec. 1966, p. 91. S. M. Irving, K & Photoresist Seminar Proc., vol. 2, 1968, p. 26. W. E. Rudge, W. E. Harding, and W. E. Mutter, Flys eye technique for generating semiconductor device fabrication masks, IBM f . Res. Dmelop., vol. 7, 1963, p. 146. A. Rogel, Durable Cr masks for photoresist applications, Reo. Sci. Instrum., vol. 37, 1966, p. 1416. A. E. Brennemann, A. V. Brown, M.Hatzakis, A. J. Speth, and R. F. M. Thomley, Two interconnection techniques for large-scale circuit integration, IBM f . Res. Dmelop., vol. 11, 1967, p. 520. [57l G. R. Brewer, The application of electron/ion beam technology to microelectronics, IEEE Spectrum, vol. 8, Jan. 1971, pp. 23-37.

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1403 metal silicon device technology, Solid-State Electron., vol. 11, 1968, D. 1105. i.F. Miller, Controlled collapse reflow chip joining, IBM I . Res. Develop., vol. 13, 1969, p. 239. F. W. Shallcross, W. S. Pike, P. K. Weimer, and G. M. F r y m a n , A photoconductive sensor for card readers, IEEE Trans. Electron Devices (Corresp.), vol. ED-17, Dec. 1970, pp. 10861087. P. M. Schaible and L. I. Maissel, Thin film maximum thermometer, Thin Solid Films, vol. 3, 1969, p. 277. S. Middlehoek, Metallization processes in fabrication of Schottkybamer FETs, IBMJ. Res.Deoelop., vol. 14, 1970, p. 1 4 8 . S. R. Ovshinsky, Reversible electrical phenomena in disordered structures, Phys. Rev. Lett., 21,1968, p. 1450. vol. T.W. Hickmott, Electroluminescence, bistable switching and dielectric breakdown of Nb,O, diodes, J . Vol. Sei. Technol., vol. 6, 1970, p. 828. L. V. Gregor, Electrical Conductivity of polydivinylbenzene films, Thin Solid Films, vol. 2, 1968, p. 235. W. E. Engeler, J. H.Tiemann, and R. D. Baertsch, Surface charge transport in silicon, A&. Phys. Lett.,vol. 17, 1970,p. 469. B. D. Josephson, Possible new effects in superconductive tunnelling, Phys. Lett., vol. 1, 1962, p. 251. J. Matisoo, The tunneling cryotron-A superconductive logic element based on electron tunneling, Proc.IEEE, vol. 55, Feb. 1967, pp. 172-1 80. W. S.Boyle and G. E. Smith, Charge coupled semiconductor devices, Bell Sysr. Tech. J., vol. 49, 1970, p. 587. A. H, Bobeck, Properties and devices applications of magnetic domains in orthofemtes, Bell Syst. Tech. J., vol. 4 6 , 1967. P.I. Bonyhard, I. Danylchuk, E. D. Kish, and J. L. Smith, Applications of bubble devices, IEEE Trans. Magn., vol. MAG-6, Sept. 1970, pp. 447451. P. Brody andD. Page, Flexible thin-film transistors stretch performance, shrink cost, Electronics, vol. 41, 1968, p. 1 0 0 .

[SEI S. M. Angello, Should microelectronic processing be done with electron beams, presented at WESCON, Sept. 1969. [59] M. J. Beesley, H. Foster, and K. G. Hambleton, Holographic projection of microcircuit patterns, Electron. Lett., vol. 4, 1968. [a]D.L. Klein and J. W. Raniseski, Photomasks and photolithography, presented at AlChE Meet., Atlanta, Ga., Feb. IS, 1970. [61] W. VanGelder and V. E. Hauser, J. Electrochem. Soc., vol. 114, 1967, p. 869. [621 C. S. Murphy, Electron Reliub. Microminiutw., vol. 2, 1963, p. 235. [63] M. K. Stetler, Chrome masks-The ideal master for photoprocessing, Solid State Technol., vol. 9, Mar. 1966, p. 60. [64] T. W.OKeeffe and R. M. Handy, Fabrication of planar silicon transistor without photoresist, Solid-State Electron., vol. 1 1 , 1968, p. 261. [65] R. F.Thornley and T. Sun, Electrical beam exposure of photoresists, J. Electrochem. SOC., vol. 112, 1965, p. 1151. [66] P.D. Davidse, RF sputter etching-A universal etch, J . Electrochem. Soc., vol. 116,1969, p. 1 0 0 . [67] L. I. Maissel, C. L. Standley, Jr., and L. V. Gregor, to be published. [68] S.W. Ing, Jr., R. F.Momson, L. L. Alt, and R. W. Aldrich, Gettering of metallic impurities from planar Si diodes, I . Electrochem., Soe., vol. 110, 1962, p. 533. [69] F.Woitsch, Silicon nitride etching, Solid State Technol., vol. 1 1 , no. 1, 1968, p. 29. [70] M. M. Schlacter, E. E. Schlegel, R. S. Keen, Jr., R. A. Lathlaen, and G. L. Schnable, Advantages of vapor-plated phosphosilicate films in large-scale integrated circuit arrays, IEEE Trans. Electron. Devices, V O ~ .ED-17, Dec. 1970, pp. 1077-1083. [71] L. V. Gregor, P. Groswald, and R. A. Powlus, Effects of sputtered Si02 on MOS integrated circuits, to be published. [72] P. Richman, Suppression of parasitic thick-field conduction mechanisms in Si-gate MOS integrated circuits, Electron. Lett., vol. 7, 1971, p. 12. [73] D. M. Brown, W.E. Engler, M. Garfinkel, and P. V. Gray, Refractory

[74] [75]
~~

[76] [77] [78] [79]


[EO]

[El] [82] 1831 1841 [E51 [86] [87]

Multilayer Metallization forLSI


C. J. SANTORO
AND

D. L. TOLLIVER

Abstract-Recent advances in the manufacture of complex bipolar A class of problems related the to presence of via holes or oxide integrated circuitshave led t o a variety of techniques for metal inter-windows for interlayer continuity presented. In addition. the probis connection on the chip. As the need for more and more devices has lem of random defects such as pinholes and inclusions in the oxide increased chip size, theproblemofrandomdefects has become insulations layers is mentioned. Finally. these data are related to the catastrophic. Functional yields are often seen t o drastically decrease tradeoffs that occur in building up additional layers or increasing die or even vanish with attempts t o fabricate very large bipolar parts. size. Since the major factor determining die size is the metal interconINTRODUCTION nect site and spacing, one way t o conserve real estate while achievHE DEMANDS of highly sophisticated electronic systems ing highly complex circuits is t o employ more than a single layer of interconnection metal. present At both doubleand triple-layer have pressured the semiconductor industry into placing more schemes are being used. Thesemultilayer metallizations, while solving and more deviceson a singlechip. This has resulted in a largethe problem of chip defects, are not without serious drawbacks of scale integration (LSI) of previously hybrid designs and led to the their own. These problems are discussed. emergence of enormous sizes. The process engineer has die seen this The Motorolamultilayer systems considered are allaluminum based; i.e., pure aluminumor lightly doped aluminum. Although other new complexity result in drastically reduced circuit probe yieldsat a metals are beingexperimented with, aluminum systems make up less time when circuits per waferare available [ 1 [2]. If one assumes nearly all of the commercially available ICs at this time. In general, that random statistics apply(usuallyaworstcase),then circuit these metal layers are insulated from one another by a deposited diyields can be expressed electric, usualty SiO,. The most prominent yield limiting problemsare discussed. These Yv = (1) edges and oxide steps with additional include coverage of both metal = (1 - a@. (2) metal and/or another layer of oxide. Processing parameters such as profiles, thickness, temperature,composition, etc., thatinfluence Here (1) relates yield to complexity, and & is the yield of the coverage are discussed as well as innovations for improving less-thancircuits building block (i.e.,transistors, gates, etc.). N is the level of desirable results.

1,

(KY

r,

Manuscript received February 18, 1971; revised April 14, 1971. The authors are with the Integrated Circuits Center, Mesa, A r k 85008.

integration; the number of such building blocks integrated into a single chip. Applyingthis relationship to a logic array, for example, shows how circuit yield and gate yield correspond. Reasonable cir-

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